Process of nitrating toluols containing paraffins.



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BERNHAIBID JACQUES FLURSCHEIM, OF FLEET, ENGLAND, ASSIGNOR T0 AETNA EXPLOSIVES COMPANY, INC. OF NEW YORK, N. Y., A CORPORATION OF NEW YORK.

PROCESS OF NITRATING TOL'UTOLS- CONTAINING PARA FFINS.

No Drawing.

Toluols Containing Paraflins, of which the. following is a full, clear, andexact descrip tion.

The object of my invention is to nitrate toluol containing paraflins and more particularly to treat the mononitro derivative thereapplicable to other hydrocarbons of the ben-* 201 series and especially to the manufacture of dinitrobenzol.

' The manufacture of trinitrotoluol from t'oluols containing parafiins has heretofore been carried out in the following way:

The toluol is nitrated to mononitrotoluol, the mononitrotoluol is separated from the parafiins by distillation, and the mononitrotoluol thus obtained freed from paraflins is nit-rated to trinitrotoluol.

This process is expensive, complicated andwasteful, as it involves acid-free washing of the mononitrotoluol before it is ready for distillation Moreover, any higher nitro compounds presentin the mononitrotoluol are lost in the shape ofstill-residue during such distilla-' they have not-satis actorily accomplished theresults attained in the practice of my invention.

I take a toluol containing 13 per cent. of

Specification of Letters Patent.

Patented May 8, 1917.

, Apnlication filed March 23', 1916. Serial No. 86,180.

paraflin andshowing the following distillation record:

First drop 109. 3 2%% 110. 5 5% 110. 7 95% 111.3 97-%% i 111.4: Dry 111.4:-

. 852 The toluol is then nitrated to mononitro- Specific gravity toluolin the following manner; 60.5 pounds of in such manner as to separate therefrom a the contained parafiins. The process is also.-

of this toluol (containing therefore 52.5 pounds of pure toluol) are run intoa nitrator and 133.8 pounds of mixed acid (one part of' 74.7 'per cent. nitric acid and l.5 parts of 96 per cent. sulfuric acid) areztlfen run-into the nitrator Within four hours with continued stirring, at a temperature gradually rising" from to C. The stirring is 1 then continued for two hours, the temperature being maintainedat 60 C. p

The mass is allowed to settle until the acid can be drawn ofl' clear at the bottom. Only the mononitrotoluol plus paraffins are left in the nitrator.

The mononitrotoluol is then separated from the contained paraffin in the following way: 138 pounds of 96 per cent. sulfuric acid are run into the nitrator all at once and mixed with the mononitrotoluol by fifteen minutes stirring. The mass is then allowed to settle for some hours, until the-bottom layer, consisting of a solution of mononitrotoluol in sulfuric acid, runs off clear. This bottom layer is drawn ofi' until the first drop of paraffin makes its appearance. The parafiins'are then drawn off separately. I

The next step is the nitration of the'puri- 'fied mononitrotoluol to trinitrotoluol. I

take (say) one half of the above solution of sulfuric acid and mononitrotoluol and add, at a temperature ofabout C., 69 parts of oleum (104 per cent.) and 109.5 parts of mixed acid containing 47.0% HNO 50.0% H SO and 3% water. The temperature is then allowed to rise at the rate of one degree in three minutes until it has reached 90 0., at which point it is kept for one hour. lit is then allowed to further rise at the rate of one degree in three minutes until a temperature of 110 .is attained, at which it'is kept for two hours. The temperature is then allowed to rise until 120 C. is reached, at which it is kept for four hours. The charge'is then run into a crystallizer.

It is unnecessary to adhere rigidly to the precise directions respecting time, temperature and proportions of materials above set out, my object in precisely setting forth a preferred way of carrying out the process being to enable those skilled in the art to practice the process without the necessity of experiment.

The above described process, with such modification as those skilled in the art can supply, is also applicable to the manufacture of dinitrobe'nzo-l, the separation from paraflins taking place, by means of sulfuric acid, in the mononitrobenzol stage. The process is also applicable to the separation of paraflins from other nononitro derivatives of hydrocarbons of the benzol series.

Having now fully described my invention,

What I claim and desire to protect by Letters Patent is:

1. The process of separating mononitrotoluol from contained paraffins which con-' sists in mixing the same with sulfuric acid until the mononitrotoluol is dissolved there- ,in and then separating the solution from the paraffins.

2. The process of separating mononitrotoluol from contained paraflins which consists in mixing the same with a substantially equal quantity by volume of sulfuric acid, and then separating the solution of mononitrotoluol and acid from the paraflins.

3. The processof manufacturing trinitrotoluol from toluol containing parafiins, which consists in nitrating the toluol to mononitrotoluol, then mixing the mononitrotoluol with sulfuric'acid until the mononitrotoluol is dissolved therein and separating out ,the undissolved paralfins, and then nitrating' the purified mononitrotoluol to trinitro-- "of, then mixing the said derivative with sulfuric acid until the said derivative is dissolved therein and separating out the undissolved paraliins, and then nitrating the purified derivativeto a higher degree of nitration.

In testimony of which invention, I have hereunto set my hand, at New York, N. Y.,

on this 17 day of March, 1916.

'BERNHARD JACQUES FLURSCHEIM.

Witnesses:

LAURA B. PENFIELD, JOHN F. HEFFERMAN. 

